Dispersion of bituminous materials and process of making same



June 16, 1925. 1,542,035

M. R. CONE DISPERSION OF BITUMINOUS MATERIALS 'AND PROCESS OF MAKING SAME Filed May 30, 1923 INVENTOR ATTORNEY Patented June 16, 1925.

' MARK R. cone, or BALTIMORE, MARYLAND, AssIeNo To THE Union TRUsT oom- PANY, or CLEVELAND, 01110, A ooRroRATIoN or OHIO.

DISPERSION OF BITUMINOUS ,MATERIALS AND PROCESS OF MAKING SAME.

Application filed May 30, 1923. Serial No. 642,372.

To all whom it may concern:

Be it known that I, MARK R. CONE, acitizen of the United States, and resident of Baltimore, and State of Maryland, have invented certain new and useful Improvements in Dispersions of Bituminous Materials and Processes of Making Same, of which'the following is a specification.

This invention relates to: a process for the treatment of bituminous materials to render the same completely miscible in Water without the admixture of any emul sifying agents, such as caustic soda'or other alkaline substances.

Bituminous materials, such as natural, residual and artificial asphalts, and asphaltic materials, such as petroleum residues and oxidized petroleums, with or without oil fluxes which are'sometimes combined with 2 resins, are extensively employed for coatings and. binders. In using these -bit uminous substances and. in making same available for ready application they have been either heated to a sufiicient temperature to admit of proper spreading or else thinned with animal, vegetable or mineral oils, more particularly the lighter hydrocarbon oils.

The inconveniences and expense incident to the heating and-the losses occasioned by .volatilization of the dissolving liquid and the expense of bringing the bituminous inaterial in the proper state of solution have made it highly desirable to devise a product wherein the bituminousematerial will be in 85 -a condition that will permit the same to be spread at ordinary temperature upon the surface to be covered without local heat treatment .or the use of these organic solvents or thinners. To. accomplish this, it 40 has been recognized of late years by numerous persons engaged in the-art that if the bituminous material could be brought into c a fine state of subdivision and in proper admixture with a cheapafluid,-such as water, so that thelresulting mixture would possess the proper mobility by-reason of the bituminous material being in a proper state of dispersion, that the disadvantages incident to the prior uses of the bituminous materials and to their former conditions would be largely overcome.

Various attempts havebeen made to solve this problem. Among these may be mentioned the addition of a colloid, such as tannic acid, to the water and the incorporation of finely ground, solid bituminousmaterial with the aqueous colloid solution. In such a mass, the particles of bituminous material become coated' with the protective colloid which prevents or retards their coalescence into a continuous mass.

In other attempts to solve this problem, caustic alkalies, such as NaOH, have been used for treating the bituminous material, but these have also proved unsatisfactory. I l Many attempts to dispense with the use of the caustic alkalies and colloids have also been made and consist in the adclitionof liquid'bituminous material to water, while agitating the mass. I proved not only unreliable but unsuccessful ,and such processes have not produced a satisfactory product having .the bituminous material properly dispersed in the aqueous medium with the particles of bituminous material remaining uncoalesced for any long. period. The failure of these prior attempts to give satisfactory results may be explained -as follows:

VVhen the I fluid bituminous material is introduced into the bath of cooler water, the molecules coming in direct, immediate contact with the bath are cooled to the temperature of the bath and become, set; The fluid bitumen not in direct, immediate con- ,tact with the bath will maintain its fluid condition until by'conduction it is cooled to a settingtemperature, and it the bath is stationary the bituminous material will deposit ip practically a continuous mass in 'the liquid and remain in a state "of immiscibility with the bath ofliquid. If, however, the bath is in a state'of nniform motion, on

reaching the bath,.the molecules of the fluid bitumen in direct, immediatecontact withthe bath will become set and carried along by the moving bath. The other portion of the fluid bitumen not in: direct, immediate. with the bath will, as long as,the'

contact proper condition of fluidity exists, allow the 'moving'bath of liquidto draw and pull and thus attenuate the bitumen into films,-

laminae or threads, depending upon the v I character of the motion of the liquid. This Y- Y.

spread while at ordinary atmospheric temperature upon the surface to be covered, such as a roof, a wall or a roadway in a layer or a plurality of layers of any desired thickness without local treatment or the application of heat or any change whatever except the addition of a sufiicient quantity of water to produce the desired flow of the material.

Among the objects of this invention is to provide a process whereby the particles of bituminous material'are dispersed in water and of such size, shape and condition as to admit of their remaining in an isolated and uncoalesced state with respect to each other for any period desired, which stateof dis-.

sociation and non-coalescence will remain undisturbed while the material is in transit I or storage and which state becomes readily disturbed when the aqueous mater al. is removed therefrom, such as on exposure to evaporation in the atmosphere, therebyresulting in a coalesced mass of continuous bituminous material.

A further object of the invention is to provide a product in the form of a bituminous paste or cement that is semi-solid and plastic, capable of being maintained in this condition for indeterminate periods of time and of being spread in layers or formed into shapes in molds or dies, which will coalesce upon being subjected to distillation or evaporation to form a compact, coherent and durable substance possessing substant'ially all the qualities inherent in the material from which it was originally formed. Furthermore, the invention consists in the new and riovel details and features of operation and the novel combinations and ar-' rangements of steps in the process for the treatment of bituminous substances hereinafter set forth and'olaimed.

In carrying out this invention, I first provide a bath of water and add thereto bituminousmaterial,, such as asphalt in fluid state, while subjecting the bath to suitable motion and agitation. By this motion the liquid comprising the bath is linearly accelerated, so that each unit portion of the liquid having the accelerated velocity will move faster than its succeeding portion, and will eventually be separated therefrom. If such liquid is in contact with the fluid invention.

bitumen, the movement of these adjacent liquid portions away from each other will exert a pulling or drawing action upon the adjacent portions of fluid bitumen in contact with the liquid, severing such portions of bitumen continuously from each other and thereby exposing a fresh portion of the fluid bitumen to contact with the liquid of the bath. This continuous severing of the adjacent portions of bitumen from each other and the bringing of fresh fluid bitumen in contact with the body of liquid results in rapid attenuation of the fluid bitumen and in ultimate comminuation thereof into finely divided particles. This atomization of the bitumen may be carried on so as to produce particles of microscopic and even colloidal size.

By producing such a high degree of attenuation, subdivision and comminution of the bitumen, the surface of the particles of bitumen acquire a greater afiinity and attraction for the water than for the other particles of bitumen, thereby counteracting the natural tendency of the particles of bitumen to coalesce with each other and conditioning the bitumen to exist in this finely divided state in the aqueous medium. The particles of bitumen are isolated from each other, the films of water serving as an insulating medium between the individual particles, opposing their agglomeration and coalescence. Y

The velocity and character of the motion of the bath is one of the important features; of this invention. The incoming material. must be subjected promptly, before it is set, to a continuous and'multi-pulling and attenuating action operative to draw or pull out the material into fine threads, laminae or films, which action must be continueduntil the attenuated product is broken up into fine particles of an elliptical or globular form instead of pieces having sharp edges of points. This pulling and attenuating action is effectively produced by a whirling motion of the bath that forms a vortex at or near its center, in which the material approaching and passing through the vortex has considerably greater speed of movement than thematerial at or near the periphery of the bath. This characteristic motion to the body of the bath may be imparted in any I desired manner, for example, by a propeller having blades of the proper angle and pitch.

The regulation of the temperature of the bath and that of the incoming bituminous material is also one of the features of my These temperatures must be regulated within comparatively narrow limits for anyparticular bituminous material, but the optimum temperature limitations of the incoming bitumen and bath vary with different bituminous materials. The temperature of the incoming bitumen is higher than that of the bath of water, and the temperature of the latter s ould be such-that when the bituminous material is cooled to the temperature of the bath itvwill have become properly set to admit of its further handling Without the particles becoming coalesced or agglomerated.

The attenuation and subdivision takes place during the period-of-transition of the bitumen from its temperature at introduction of that of setting. This transition period is of very short duration, and it is, therefore, necessary for the attenuation and subdivision of the bitumen to be accomplished in such short period, which begins from the instant the bitumen is introduced into the bath.

Another feature of my invention consists in the proper positioning of the rotating agitator or propeller in the bath. Not only is it necessary that the proper attenuation and subdivision be accomplished in the bitumen, but in order to obtain a suitable and desirable product it is also necessary that all of the bitumen be given this treatment and transformation. Otherwise, onlya partial attenuation and subdivision will take place and the bitumen which has not been given such treatment and transformation will not only impair the product because of the agglomeration and coalesced masses therein but will operate to bring about coalescence of the otherwise non-coalescing particles. By suitably adjusting the propeller so that the liquid at the surface is drawn into a rapidly moving accelerating vortex and then dispersed into a more slowly moving body of zone of the bath, I obtain a compound motion of the liquid of the bath resulting in all of the liquid being sub: jected at very short intervals to the varying linear velocities in the various parts of the bath. a

To practice the process successfully it is necessary to preserve a proper relationship between all of the above factors, each of which appears'to be almost equally important toward obtaining a product possessing the requisite and necessary characteristics. By adjustingthe temperatures of the bath and incoming fluid bitumen so that their difference'in temperature will admit of proper attenuation and subdivision of the bitumen during the transition period and delivering the incoming fluid bitumen to; the bath so that it will be subjected promptly to the pulling effect of the accelerated velocity of the moving liquid produced by adjusting the position, speed and pitch of the propeller or rotating agitator, the bitumen will be dispersed into fine particles in the liquid, which particles under microscopic examination show curved outlines of spheroidal orellipsoidal shapes and have such a very high affinity for the water that they are attracted If, however, the process is not properly practiced and if the various factors embodyin'g the features of my invention are not properly coordinated so that during the transition period the bitumen is not properly attenuated and subdivided because the cooling has been too rapid or too slow due to an' improper temperature of the bath or an insufficient difference of temperature between the bath and incoming fluid bitumen, or because there has been an insufficient speed or imp-roperfluidity of the bath, or a failure! to subject the incoming fluid bitumen to the zone of the bath. having the accelerated linear velocity or an improper positioning or pitching of the propeller or rotating agitator, there will be produced in the mass either no substantial comminution of the bitumen or else there will be varying amounts of agglomerated masses and particlesof finely divided bitumen, which under the microscope show, not spheroidal or ellipsoidal forms, but particles with edges and points, more or less defined, which points and edges operate to puncture the films of liquid enveloping these particles, thereby promoting fusion, agglomeration and coalescence of the particles.

In carrying out this -invention, starting with water as a bath and with bituminous material such as asphalt in a fluid state, the aqueous bath is gradually built up to meet the conditions of satisfactory and eflicient working operation. At "the start, the viscosity of the water bath is relatively low to that of the bath \under 1 proper working conditions and a relatively lower propeller speed will sufiice. Also, in order that the proper dragging, pulling and attenuating effect be produced on the fluid bitumen which is delivered to the bath, the viscosity of the incoming fluid bitumen should be maintained at a rela:

tively low point,- and as the viscosity of the bath increases the fluid bitumen-may also have a higher viscosity.

.The temperature of the Water bath is regulated according to the character of the .ing, the incoming fluid bitumen is of lower viscosity and therefore at a higher tom perature than that employed afterthe process is fully operative, and the waterbath may, therefore, be at a correspondingly higher temperature than during regular operation and, at the same time, provide the proper difference in temperature between the incoming fluid bitumen and the bath.

' As the viscosity of the bath increases, that of the incoming fluid bitumen may also be found convenient to build up the viscosity of the bath by the addition of some inert substance, such as clay, or other finely divided solid substance, or by the addition of neutral animal or vegetable oils, which do not have a solvent action on the bitumen, because these additional inert substances permit greater latitude in the range of variation of the several factors incident to this process. Ifclay is employed, it may vary from a trace to about of the amount of bituminous material.

The run may also be started by taking some of the finished product and stirring it up in water, until a bathof the desired viscosity is obtained, and raising this bath to the proper 1 temperature relative to the incoming bitumen. After the bath has been built up to the proper condition, the process may be continued indefinitely by supplying suitable quantities of fluid bitumen and water with or without the addition of any viscosity-increasing, inert substances.

As a specific example of practicing my invention on a commercial scale, themethod of treating by my process a standard and well-known material, for example, the asphalt known as standard asphalt macadam binder C, produced from heavy Mexican crude oil at the Baltimore refinery of the Standard Oil Company of New Jersey will be illustrated. -An' analysis of this material is as follows:

Specific gravity at F Weight per gallon at 60 F 8. 68 lbs. Flash point (open cup) 470 F. Melting point (Ballet Ring) 118 F. Penetration 77 F Penetration 32 F 26 Penetration F Volatility of 20 grams in 5 hrs. at

325 F 05% -Penetration of residue 71 Ductility 80 plus. Soluble in carb. bisulphide 99.8% Soluble in 76 naptha 77.1% Fixed carbon 15. 0%

The asphalt is first heated to a temperature of 250 to 275 F. in'any suitable apparatus, such as a standard type of melt-' ing tank or jacketed kettle The bath, which may consist of previously treated material, is held in a suitable container, for instance, a standard jacketed circular tank or kettle, provided with a propeller or agitator, having blades approximately one-third the radius of the tank or kettle, and set at a pitchthat will produce the special movement of the bath hereinafter described.

The bath is heated to a temperature of approximately 110 F., and the propeller is set in motion so as to cause the mass of the bath in the upper portion of the container above the propeller to move in a direction from the outer wall of the container toward the axis and downward, and to travel in a reverse direction in the lower portion of the container below the propeller. The movement of the bath in the upper portion of the container above the propeller is one of acceleration from the outer circumference of the container to the axis and downward to the propeller, thereby forming a vortex, and from a point between the circumference and the axis, usually approximately one half Way, this acceleration of the bath in- -creases greatly and the movement becomes ,very rapid. v

J The liquid asphalt is supplied as needed,

preferably continuously and in suitable quantities, to the bath in a stream or streams, such as a spray, for example, about one-half way between the circumference and the axis of the container and in the upper portion of the container above the pro peller. As the dispersion of the asphalt in the bath proceeds, the temperature of the bath tends to increase and the viscosity of the bath also increases. The temperature may be permitted to increase until it reaches approximately F., when preferably any further increase in temperature is checked in a suitable manner, as by circulating cooling water through the jacket of the container. As the viscosity of the bath increases, water is added from time totime' in suitable volume to maintain the fluidity of the bath within such limits that the proper movement of the bath as herein described will take place without material deviation. The temperature of the incoming water is regulated so as not to vary substantially the temperature of the bath.

In the accompanying diagrammatic drawing I have illustrated diagrammatically the apparatus employed in carrying out my improved process, in which a container or jacketed kettle a is provided with a propeller 0 driven in any suitable manner, as by a shaft 2), whereby the vortex may be produced in the material being treated. This vortex is indicated by dotted lines, but it will be understood that it is impractical to show accurately the exact path of any particles in the material through the vortex, nor is it necessary for the material to follow any such precise and defined path in standard forms of receptacles or kettles may be employed, and that the form, proportions, position and speed of the propeller may be varied, provided only a definite vortex is produced in which the asphalt is subjected to a pulling and attenuating movement at the proper temperature and for the appropriate period of time sulficient to break up and disperse into particles of the desired fineness the incoming bituminous or other material.

The total volume oi the bath is preferably maintained approximately constant by removing from time to time or in a continuous manner a quantity of the bath, after it carries a sufiicient amount of dispersed asphalt, in volume equal to the combined volume of the incoming asphalt and water. This dispersion of asphalt may be a discharged into storage vessels or containers for further cooling, and constitutes the finished product of the process.

The dispersed asphalt in the water which is removedfrom the bath may be. allowed to settle and any excess, supernatant liquid isremoved by decantation or any other suitable means. removing the supernatant liquid has the appearance of a semi-liquid, finely grained,

somewhat oleaginous paste in which the. larger particles are visible to the naked eye.

The water forming the dispersion medium for the dissociated-and dispersed bituminous material, having particles approaching.

colloidal size, is deeply colored as a result of such dispersed particles in suspension. This paste is very stable in character and will maintain its characteristics indefinitely unless the moisture is removed from the mass by distillation, evaporation or in some similar manner, when the particles will coalesce to form a homogeneous body of the bituminous material similar in practically all respects as to chemical analysis and physical characteristics to the original substance prior to treatment.

' When the paste is spread out in a layer -or coating, however, the moisture evaporates and thereupon the particles coalesce to form a continuous, coherent and homogeneous layer possessing substantially all of the properties and characteristics of the original bituminous substance and forming a close, compact, coherent body or layer particularly adapted to form a surface coating especially for roadways and places where resisting qualities are required.

It is not essential that the water supplied to the bath be free from suspended solid matter, provided such solid matter is chemically neutral and inert with respect to the asphalt, said solid matter serving merely as a filler or extender in the finished product. If such a filler or extender is desired in the finished product, it may be added to the The mass which remains after bath with the water of dispersion or in any other suitable manner and in such'quantity as may be desired. It will also be obvious that where s ecial products aredesired that particular substances, for example, inert materials such as pigments, may be added to the bath. together with the asphalt 'and water so as to become incorporated with or distributed through the bath and thus become part of the final product.

This invention may be applied to the preparation of dispersions of many liquefiable substances in liquids ordinarily immisci'ble therewith. These include the general class of bituminous materials, of native and artificial origin and also the pitches derived from the tars and tar'products obtained in the various industries, the oil pitches obtained-in the distillation and cracking of animal, vegetable and petroleum oils of asphalt, paraifine, naphthene or other base and those pitches resulting from destructive distillation of organic matter of animal, vegetable or mineral origin.

This invention contemplates the treatment of bitumens and other liquefiable substances heretofore described of high or low melting points. If the bitumens or other substances which are fluid at ordinary temperatures are treated, the aqueous bath is cooled in order to provide the proper dif ference in temperature between the incoming fluid bitumen or other substance and the bath and the proper cooling of the particles to bring about their proper setting. Likewise, in the case of bitumens or other substances of high melting point, if it is desired to have the aqueous bath at temperatures above 212 F., suitable materials may be added to raise the boiling point.

This invention also contemplates the dispersion ofthe bitumen or these other substances in liquids other than water, which do not have a solvent action on the material being dispersed and "which will have a greater afiinity for the particles of finely divided material than the particles have for each other.

This invention is adapted to the manufacture of. dispersed bituminous and other materials -with particles of various sizes, and the degree of dissociation may be car ried to the extent of producing particles of approximately collodial size. Other things being equal, increase of speed and prolongation of the period during which the incoming fluid material being dispersed is brought to the setting temperature, results in greater attenuation and a finer subdivisionof the It will be understood that the term bituminous material, as used by me, is inspecify the bituminous material is introduced into the zone of the moving liquid, I intend to include the immediate vicinity of such zone which, for the purposes of my process, "will give approximately the same results.

The present invention is not limited to the specific details set forth in the foregoing examples which should be construed as illustrative and not by way oflimitation, and in view of the numerous-modifications which may be effected therein without departing from the spirit and scope of this invention, it is desired that only such limitations be imposed as are indicated in the appended claims.

I claim as my invention:.

1. Ina process of dispersing .a herein described heat liquefiable substance inaliquid ordinarily immiscible therewith,- the steps which include subjecting said substance in a fluid state to tension and accelerated motion in the presence of said liquid. v,

2. In a process of dispersing a herein described heat liquefiable substance inaliquid ordinarily immiscible therewith, the steps which include subjecting said substance in a fluid state and in the presence ofsaid liquid to tension, accelerated motion and progressive severing of its constituent particles.

3. In a process of dispersing a herein described heat liquefiable substance in a liquid ordinarily immiscible therewith, the steps which include subjecting said substance in I a fluid state to high tension and progressive severing of; its constituent particles into minute, non-coalescing globules by the action of said liquid moving with an accelerated velocity. ,I

4. In a process of dispersing bitumi-nous material in water, the steps which include subjecting said bituminous material in a fluid state to accelerated motion and high tension by the action of water moving with accelerated linear velocity.

,5, In a process of dispersing. bituminous material in water, the steps which include subjecting said bituminous-material 'ina fluid state and in th'e presence ofthe water to tension, acceleratedmotion and progre's'} sive-severing of its constituent particles.

6. In a process of dispersing bituminous material in a liquid ordinarily immiscible therewith, the steps which include subject ing said bituminous material in a fluid state to high tension and progressive: severing of its constituent particles into 'in1nute,noncoalescing globules by the action of said I liquid moving with an accelerated velocity.

. as to be immediately propelled by the moving liquid into the zone where the liquid is moving at an accelerated velocity.

9. 1A process comprising introducing a herein described heat liquefiable substance inr a fluid state into a bath of moving liquid ordinarily immiscible therewith in th immediate vicinity of the zone where the bath of liquid is moving at an accelerated velocity, adjusting and maintaining the temperature of the bath to admit of high degrees of attenuation and dispersion before the substantial solidification of said liqueflable sub-stance.

10. A process comprising introducing fluid b-itumino usainaterial into a bath of moving liquid ordinarily immiscible therewith at such zone where the liquid is moving at an accelerated velocity, adjusting and maintaining the difference in temperature between the bath and the incoming fluid bitumen to admit of high degrees of attenuation and dispersion before the su stantial solidification of said bitumen.

11. A process comprising introducing fluid asphalt into a moving, aqueous bath. at such zone where the water is moving at an accelerated velocity, adjusting and maintaining the difference in temperature between the bath and .the incoming fluid asphalt to admit of high degrees of at tenuatioli anddispersion before the substantial solidification of said asphalt.

12. A process comprising introducing fluid bituminous materialinto a bath of rotating'liquid ordinarily immiscible therewith in the immediate vicinity of the zone where the liquid is'moving at an' accelerated velocity, adjusting and maintaining the difference in temperature between the bath and the incoming" fluid bitumen to admit of high degrees of attenuation and dis persion before the substantial solidification of saidbitumen.

, 13. A process com-prising introducing fluid bituminous material into a bath of moving liquid ordinarily immiscibletherefine particles. a

14. A process comprising introducing 20. In a process of dispersing bituminous a liquefiable substance inwa fluid state into material in a liquid ordinarily immiscible a cooler bath of a liquid ordinarily immiscitherewith, introducing the bituminous mable therewith, subjecting said fluid substance terial into a bath of said liquid, maintainto the immediate action of attenuating ing the bath at temperatures where the biforces comprising a powerful drawing actuminous material introduced therein will tion by said liquid and dissociating said have fluidity admit-ting of high degree of fluid substance intoglobules approaching attenuation when subjected to a force opcolloidal size and non-coalescent with each crating to attenuate said bituminous maother in said liquid. terial and subjecting the bath to amotion 15. A process comprising introducing a operating to bring the bituminous material liquefiable substance in a fluid state into a introduced therein under the action of the bath of moving liquid ordinarily imniisciattenuating force. ble therewith in the immediate vicinity of 21. In a'process-ofdispersing bituminous the zone where the liquid is moving at an material in a liquid ordinarily immiscible accelerated velocity, said bath of liquid betherewith, introducing the bituminous maing subjected to a compound motion reterial into a bath of said liquid, maintain sulting in all of the liquid undergoing, at ing the bath at temperatures where the bivery short intervals, the varying linear vetuminous material introduced therein will locities in the various parts of the bath. have fluidity admitting of high degree of 16. A process comprising introducing attenuation when subjected to a forc opfluid bituminous material into a 'moving, crating to attenuate said bituminous maaqueous bath in the immediate vicinity of terial, imparting motion to the bath of said the zone where the water is m oving at an liquid and subjecting said bituminous maaccelerated velocity, said aqueous bath be-' terial to an attenuating force comprising a ing subjectedto a compound motion resu'ltdrawing action by the moving liquid bath. ing in all of the water undergoing, at very 22. In a process of dispersing bituminous short intervals, the varying linear velocimaterial in a liquid ordinarily immiscible ties in the various parts of the bath. therewith, introducing; bituminous material 17. In a process of dispersing bituminous in a fluid state into a bath of said liquid, esmaterial in a liquid ordinarily im miscible tablishing a transition period by adjusting therewith, introducing the bituminous mathe temperature of the bathipthat of the terial into a bath of said liquid,.maintainincoming bituminous fluid dur'ng which peing the bath at temperatures where the riod said bituminous fluid is cooled from its bituminous material introduced therein will incoming temperature to that of the bath, have fluidity admitting of high degree of imparting motion to the bath of said liquid attenuation when subjected to a force opand subjecting said bituminous fluid during crating to attenuate said bituminous mathe transition period to an attenuating force terial and subjecting said bituminous macomprising a drawing action by the moving terial to the attenuating f rce. liquid bath.

' 18. In a process of dispersing bituminous 23. In a processof dispersing bituminous material in water, introducing the bituminmaterial in a liquid ordinarily immiscible ous material into a bath of water, maintaintherewith, introducing bituminous material ing the bath at temperatures where the biin a fluid state into a bath of said liquid, estuminous material introduced therein will tablishing a transition period by adjust have fluidity admitting of high degree of ing the temperature of the bath to that of attenuation when subjected to a force opthe incoming bituminous fluid during which crating to attenuate said bituminous maperiod said bituminous fluid is cooled from terial and subjecting said bituminous maits incoming temperature to that of the bath, terial to the joint action of the attenuating impart-ing motion to the bath of said liquid force and a force operating to dissociate by means ad usted within said bath and opthe attenuated bituminous material into crating at suflicient velocity to draw during the transition period all of the bituminous 19, I a proce s f di p r i g bit i s flu'id introduced into the bath into the material in a liquid ordinarily immiscible sphere of attenuation and dispersion. therewith, introducingthe bituminous ma- 4'- II a process of dispersing bituminous terial into a bath of said liquid, mainta'iiimaterial in a liquid ordinarily immiscible ing the bath at temperatures and visdosity therewith, introducing the bituminous maher th bit i u mat rial introduced terial into a bath of said liquid, maintaintherein will have fluidity admitting of high ing the bath at temperatures where the bidegree of attenuation when subjected to a tuminous material introduced therein will Iorce operating to attenuate said bituminous have fluidity admitting of high degreeiof atmaterial and subjecting said bituminous tenuation when subjected to a force operat- L material to the attenuating force. ing to attenuate said bituminous material,

ioo

impartin accelerating motion to the bath of said liquid and subjecting said bituminous material to an attenuating force comprising a drawing action by the moving liquid bath.

25. In a process of dispersing bituminous material in a liquid ordinarily immiscible therewith, the steps which include subjecting the bituminous material'in a fluid state to high, increasing tension and accelerated motion in the presence of said liquid.

26. In a process of dispersing a liquefiable substance in a liquid ordinarily immiscible therewith, the steps whichinclude subjectingsaid substance in a fluid state to high, increasing tension and motion having increasing acceleration in the presence of said liquid.

27. In a process of dispersing a liquefiable substance in a liquid ordinarily immiscible therewith, the steps which include subjecting said substance in a fluid state to high, increasing tension and motion having increasing acceleration by the action of said liquid moving with a velocity having increasing acceleration.

28..A bituminous dispersion comprising essentially finely divided particles of bitumen of curved outlines which show on microscopic examination spheriodal and ellipsoidal shapes, said particles having insulating films composed of substantially unmodified liquid ordinarily-immiscible therewith opposingtheir coalescence and agglomeration.

29. A bituminous composition comprising essentially a dispersion, in a liquid ordinarily immiscible therewith and substantially free from alkalics and protective colloids, of minute, bituminous globules in a state of isolation from each other.

30. A bituminous dispersion comprising essentially dissociated particles of bitumen of curved outlines which show on micro- 'scopic examination spheroidal and ellipsoidal shapes, said particles having adhering, insulating films of a liquld, ordinarily immiscible therewith and substantially free from alkalics and protective colloids, op-. posing their coalescence and agglomeration.

31.A bituminous dispersion comprising essentially dissociated particles of bitumenland this 28th day of May, 1923. A. D.

of curved outlines which show on microscop1c exammation spheroidal and ellipsoidal shapes, said particles having adhering, insulating films composed of water 0pposing their coalescence and agglomeration.

32. A pasty, bituminous composition, comprising essentially minute globules of bituordinarily immiscible therewith and substantially free from alkalics and protective colloids, of noncoalescing, bituminous globules in a state of isolation from each other.

34. A new article of manufacture comprising bituminous material in the form of finely divided particles, each of said particles being surrounded by a film composed of substantially unmodified liquid, the said particles forming a plastic, homogeneous mass miscible in water. I

35. As a. new article of manufacture, a plastic material comprising particles of bitumen in a finely divided state, the said particles being combined with a liquid composed of water in quantity sufiic-ient to prevent coalescence while said particles are in a moist condition and adapted to coalesce when the water is removed.

36. A bituminous composition for use as a surface covering comprising particles of bituminous material dispersed in "an agent composed of substantially unmodified liquid to form a mass of separate particles capable of being spread in athin layer to form a sur: face coating, the said particles being adapted to coalesce upon evaporation of the liquid to form a dense, hard, homogeneous layer non-miscible in water. I

37 A bituminous composition capable of use as a surface covering comprising minute particles of bituminous material dispersed substantially in the colloid state in an agent composed of substantially unmodified nonsolvent liquid, the said particles being of approximately the same consistency and composition throughout and normally prevented from coalescence by adsorbed moisture on the surface of the'particles but coalescing to form a continuous, homogeneous layer when said moisture is evaporated.

Signed at Baltimore and State of Mary- MARK' B. CON E 

